CN110157531A - A kind of Biodegradable lubricant oil and preparation method thereof - Google Patents
A kind of Biodegradable lubricant oil and preparation method thereof Download PDFInfo
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- CN110157531A CN110157531A CN201910466376.4A CN201910466376A CN110157531A CN 110157531 A CN110157531 A CN 110157531A CN 201910466376 A CN201910466376 A CN 201910466376A CN 110157531 A CN110157531 A CN 110157531A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M109/00—Lubricating compositions characterised by the base-material being a compound of unknown or incompletely defined constitution
- C10M109/02—Reaction products
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/044—Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/40—Fatty vegetable or animal oils
- C10M2207/401—Fatty vegetable or animal oils used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/08—Resistance to extreme temperature
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/10—Inhibition of oxidation, e.g. anti-oxidants
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/64—Environmental friendly compositions
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Abstract
The invention discloses a kind of Biodegradable lubricant oil and preparation method thereof, the preparation method includes the following steps: that (1) weighs each raw material: cottonseed oil, bis- (2- ethylhexyl) sebacates, dispersing agent, extreme pressure anti-wear additives, antioxidant, potassium sorbate, dodecenylsuccinic acid, viscosity index improver, defoaming agent;(2) cottonseed oil is added to and is reconciled in kettle, stirring, by 2-10 μm of filter release to get.Biodegradable lubricant oil of the present invention, formula is scientific and reasonable, to environmental-friendly, nontoxic, it is not only cheap using oil based on cottonseed oil, and be biodegradable, have the characteristics that it is environmentally protective, by the lubricity, the abrasion resistance that cottonseed oil functionalization, greatly improve lubricating oil;Preparation method simple process, easy to industrialized production, Biodegradable lubricant oil of the invention is excellent in terms of wear resistence, lubricity, low temperature properties, high temperatures, thermal oxidation stability energy, and biological degradability and economy are better than fully synthetic machine oil.
Description
Technical field
The invention belongs to technical field of lubricating oil, specifically, being related to a kind of Biodegradable lubricant oil and its preparation side
Method.
Background technique
Lubricating oil such as plays antiwear and antifriction, cooling in equipment operation and improves efficiency at the indispensable key effect, but
It is usually poor with the compatibility of environment.The biological degradability of conventional mineral lubricating oil is poor, if in production, storage and transportation and use process
Middle generation leakage just pollutes the environment.Since mineral lubricating oil biological degradability is poor, in addition enhancing and the state of people's environmental consciousness
Family environmental regulation it is stringent, the research and development of Biodegradable lubricant oil is increasingly valued by people.China market is most
Popular lubricating oil oil product is oily lubricating oil based on petroleum mostly, it is difficult to degrade, stay for a long time in the environment.The annual whole world disappears
Consume lubricating oil be ten thousand tons of 3600-4000, wherein 10,000,000 tons or so of lubricating oil due to leakage, splashing, oil gas evaporation, be packed for
The residual of product such as undeservedly abandons at the ecological environment that reasons are directly entered human living, serious contaminated soil and the water resource, destroys
Ecological environment.Currently, Biodegradable lubricant oil has become the important component part of Green Chemistry and green engineering field.
Biodegradable lubricant oil refers to the requirement for being not only able to satisfy mechanical equipment, but also can be micro- by activity in a short time
Biological decomposition is the lubricating oil of carbon dioxide and water, it is typically incorporated into the column of environmental friendly lubricant.Environmental friendly lubricant
Performance not only include biodegradability, but also the eco-toxicity including lubricant.Biological degradability and eco-toxicity are
Two different aspects, some noxious materials are also biodegradable, and non-toxic substance is generated after degradation;After some mass degradations
Product has stronger toxicity than original matter.Environmental friendly lubricant should ask biological degradability to get well, but require eco-toxicity and
Cumulative toxicity wants small.
Before earliest biological lubricant can trace back to millennium, people oneself started with animal tallow and vegetable oil
Lubricate the movement of object.The attention that ancient Egyptian lubricates wheel hub is made so that they start to lubricate olive oil calcium soap
With generation interest.Biological lubricant is properly termed as biology base environment-protective lubricant oil again, refers to being partly or fully originate from biological money
The lubricating oil of source or renewable agricultural or forest resourceies.Biological lubricant in addition to the characteristic with mineral lubricating oil, also as its
The advantages that raw material is renewable, biodegradable, small toxic action is concerned.Difference according to base oil divides lubricating oil
Class can be divided into three categories, mineral oil, synthetic oil and crude vegetal.The lubricating oil of plant oil base is a kind of environmental-friendly
Lubricating oil, such as soya-bean oil, corn oil, rapeseed oil, cottonseed oil, wherein enter market earliest is the profit that Germany is synthesized with rapeseed oil
Lubricating oil;Though crude vegetal can be directly used as lubricating oil because its oxidation stability is too poor so that its application very by
Limit.Synthetic lubricant fluid mainly includes synthesis hydrocarbon, synthetic ester, polyethers etc..Wherein the research of synthesizing ester oil is the most extensive.It shows according to investigations
Show, in Lube Oil In The World application market, the ratio of mineral oil is up to 85% or so, and vegetable oil accounts for about 2%, and remaining is synthesis
Oil.
The Chinese patent of application number 201210404795.3 discloses a kind of biodegradable lubricating oil, and feature exists
In: by base oil;Antioxidant;Rust oxidation;Anti-foaming agent;Metal deactivator;Demulsifying agent;Antiwear additive;Detersive;Viscosity refers to
Number modifier;Cupric oxide powder;Metal magnesium powder composition.The antioxidant is the mixing of diaryl-amine and dithiocar-bamate
Object;Rust oxidation is alkyl acid derivative;Anti-foaming agent is dimethylsiloxane polymer;Metal deactivator is triazole;
Demulsifying agent is the poly- phenol of poly- alcoxyl;Antiwear additive is alkyl phosphate ester-containing and salt;Detersive is calcium mahogany sulfonate;Viscosity index (VI) is improved
Agent is ethylene propylene copolymer.
The Chinese patent of application number 201510472291.9 discloses a kind of preparation method of engine lubricating oil, first takes ring
Alkyl oil, cottonseed oil, hydroxy silicon oil, potassium hydroxide and ethylene glycol mix, heating, and heat preservation reflux is let cool, in gained supernatant
Middle addition oleic acid, nano silica, microwax, zinc dialkyl dithiophosphate, methyl 2-benzimidazolecarbamate mix
Close, heating, insulated and stirred, in the resulting mixture be added triphenyl phosphite, succimide, dioctyl adipate, gather it is different
Butylene succimide, 2,3- epoxypropyltrimethylchloride chloride, 2- hydroxyl -3- sulfonic group propyl starch ether mix, heating,
Insulated and stirred to get.
The Chinese patent of application number 201610764929.0 discloses a kind of preparation method of degradable biological lubricating oil,
Include the following steps: to mix in lanolin fatty acid, sodium hydroxide, ethyl alcohol, water, be heated to 60~90 DEG C, adjusting pH value is 7~9, cooling
To 50~60 DEG C, reaction solution is obtained;Above-mentioned reaction solution is mixed with water, calcium chloride, zinc sulfate, maintains 50~60 DEG C of temperature, instead
After answering 1~3 hour, through filtering, alcohol is washed, and is washed, and drying obtains additive;On being added after castor oil is heated to 40~45 DEG C
Additive, defoaming agent and water are stated, 10~20min is stirred under the revolving speed of 35~40rps;Viscosity modifier is added, 30~
20~30min is stirred under the revolving speed of 35rps to get degradable lubricating oil is arrived.
Attention with people to quality of lubrication oil and environmental protection, by degradable vegetable oil or synthetic lubricant fluid application
It in mechanical lubrication and receives significant attention, therefore, develops a kind of environmental-friendly, degradable, and the lubricating oil of high quality comes
The deficiency for making up existing lubricating oil, development industrial to promotion are of great significance.
Summary of the invention
Of the existing technology in order to solve the problems, such as, one of the object of the invention is to provide a kind of Biodegradable lubricant oil,
Its main feature is that environmental protection, can degrade, greasy property is good, anti-wear and wear-resistant performance is good, long service life, it is more preferable to the protections of parts,
Comprehensive performance is higher, cost is reasonable, energy-saving effect is obvious.The second object of the present invention is to providing a kind of Biodegradable lubricant oil
Preparation method.
The present invention is implemented as follows:
A kind of preparation method of Biodegradable lubricant oil, includes the following steps:
(1) weigh each raw material: cottonseed oil, bis- (2- ethylhexyl) sebacates, dispersing agent, extreme pressure anti-wear additives, antioxidant,
Potassium sorbate, dodecenylsuccinic acid, viscosity index improver, defoaming agent;
(2) cottonseed oil is added to and is reconciled in kettle, stirring, by 2-10 μm of filter release to get.
A kind of preparation method of Biodegradable lubricant oil, includes the following steps:
(1) each raw material: cottonseed oil or 65-75 parts of functionalization cottonseed oil, bis- (2- ethylhexyl) last of the ten Heavenly stems two is weighed by weight
5-15 parts of acid esters, 0.2-1 parts of dispersing agent, 1-5 parts of extreme pressure anti-wear additives, 0.5-2.5 parts of antioxidant, potassium sorbate 0.005-0.025
Part, 0.005-0.025 parts of dodecenylsuccinic acid, 3-9 parts of viscosity index improver, 0.005-0.025 parts of defoaming agent;
(2) cottonseed oil or functionalization cottonseed oil are added in reconciliation kettle, bis- (2- second is added at being 65-75 DEG C in temperature
Base hexyl) sebacate, dispersing agent, extreme pressure anti-wear additives, dodecenylsuccinic acid, potassium sorbate stir 10-20min, then plus
Enter antioxidant, viscosity index improver, defoaming agent stirring 30-50min, by 2-10 μm of filter release to get.
The revolving speed stirred in the step (2) is 300-700r/min.
The functionalization cottonseed oil the preparation method comprises the following steps: being in mass ratio 1:(0.07-0.12 by cottonseed oil, ethyl alcohol) with turn
Speed is 30-50 DEG C in environment temperature after being 100-500r/min stirring 5-15min and uses radiation dose rate for 3-7kGy/h's
60Co gamma-rays carry out radiation treatment 2-5h, then temperature be 40-55 DEG C, absolute pressure be 0.005-0.01MPa decompression steam
It evaporates except ethyl alcohol, the cottonseed oil after being irradiated;By cottonseed oil, acetic acid, (the dioctylphyrophosphoric acid acyl-oxygen of isopropyl three after irradiation
Base) titanate esters, concentrated phosphoric acid be 1:(0.07-0.12 in mass ratio), (0.07-0.12), (0.003-0.005) with revolving speed for 100-
500r/min stir 5-15min, temperature be 30-50 DEG C, revolving speed be 100-500r/min stirring under be added dropwise 35-45wt% dioxygen
Water, the rate of addition of the 35-45wt% hydrogen peroxide are 0.1-0.5g/s, and the dosage of the 35-45wt% hydrogen peroxide is irradiation
The 30-35% of cottonseed oil weight afterwards after hydrogen peroxide is added dropwise, is warming up to 55-65 DEG C of reaction 3-5h, and liquid separation removes water phase,
Obtain reaction product;Reaction product is carried out being washed to pH being 6.5-7.5 with the sodium hydrate aqueous solution of 0.5-1wt%, by water
Reaction product after washing is 70-80 DEG C, absolute pressure 0.005-0.01MPa vacuum dehydration 2-5h in temperature, obtains functionalization cotton
Seed oil.
The dispersing agent is polyisobutylene succinamide and/or boronation polyisobutylene succinamide.
The antioxidant is 2,6 di tert butyl 4 methyl phenol or 4- amino -2,6 di t butyl phenol.
The viscosity index improver is polymethacrylates.
The extreme pressure anti-wear additives are n-butoxy (cyclohexylamine methyl benzotriazole) phosphate derivative and/or different octyloxy
(tridecyl primene JM-T benzotriazole) phosphate derivative.Further, the extreme pressure anti-wear additives are n-butoxy (cyclohexylamine
Methyl benzotriazole) phosphate derivative, phosphate derivative is in mass ratio for different octyloxy (tridecyl primene JM-T benzotriazole)
For 1:3 composition.
The defoaming agent is polyether-modified silicon defoaming agent.
A kind of Biodegradable lubricant oil is prepared using the preparation method of above-mentioned Biodegradable lubricant oil.
Biodegradable lubricant oil of the present invention and preparation method thereof, formula is scientific and reasonable, to environmental-friendly, nontoxic, use
It is oily based on cottonseed oil, it is not only cheap, and be biodegradable, have the characteristics that it is environmentally protective, by cottonseed oil function
Energyization processing greatly improves lubricity, the abrasion resistance of lubricating oil;Preparation method simple process, it is easy to industrialized production, this
The Biodegradable lubricant oil of invention is excellent in terms of wear resistence, lubricity, low temperature properties, high temperatures, thermal oxidation stability energy, raw
Object degradability and economy are better than fully synthetic machine oil.
Specific embodiment
Embodiment is raw materials used as follows:
Cottonseed oil is provided by Xi'an Lv Teng Biotechnology Co., Ltd, appearance: light yellow liquid, product specification: 99%.
Polyether-modified silicon defoaming agent is provided by Dongguan City De Feng defoaming agent Co., Ltd, model: DF-668.
Polymethacrylates is provided by Shanghai Ming Lan Chemical Co., Ltd., model: T819HB.
Boronation polyisobutylene succinamide is provided by Jinzhou Huifa Tianhe Chemical Co., Ltd., model C-TEC
151B。
Different octyloxy (tridecyl primene JM-T benzotriazole) phosphate derivative according to application No. is
201110365059.7 Chinese patent in the preparation of method shown in embodiment 3.
Dodecenylsuccinic acid is provided by Shanghai Ming Lan Chemical Co., Ltd., model: T746.
N-butoxy (cyclohexylamine methyl benzotriazole) phosphate derivative is according to application No. is in 201110365059.7
In state's patent prepared by method shown in embodiment 2.
Embodiment 1
The preparation method of Biodegradable lubricant oil, includes the following steps:
(1) each raw material: 70 parts of cottonseed oil, bis- 10 parts of (2- ethylhexyl) sebacates, dispersing agent 0.5 is weighed by weight
Part, 3 parts of extreme pressure anti-wear additives, 1.5 parts of antioxidant, 0.01 part of potassium sorbate, 0.01 part of dodecenylsuccinic acid, Viscosity Index improve
5 parts of agent, 0.01 part of defoaming agent;
(2) cottonseed oil is added in reconciliation kettle, bis- (2- ethylhexyl) sebacates is added at being 70 DEG C in temperature, divide
Powder, extreme pressure anti-wear additives, dodecenylsuccinic acid, potassium sorbate stir 15min, antioxidant are then added, Viscosity Index improves
Agent, defoaming agent stir 40min, are released by 5 μm of filters to get Biodegradable lubricant oil.
The revolving speed stirred in the step (2) is 500r/min.
The dispersing agent is boronation polyisobutylene succinamide.
The antioxidant is 2,6 di tert butyl 4 methyl phenol.
The viscosity index improver is polymethacrylates.
The extreme pressure anti-wear additives are different octyloxy (tridecyl primene JM-T benzotriazole) phosphate derivative.
The defoaming agent is polyether-modified silicon defoaming agent.
Embodiment 2
The preparation method of Biodegradable lubricant oil, includes the following steps:
(1) each raw material: 70 parts of functionalization cottonseed oil, bis- (2- ethylhexyl) sebacate 10 part, points is weighed by weight
0.5 part of powder, 3 parts of extreme pressure anti-wear additives, 1.5 parts of antioxidant, 0.01 part of potassium sorbate, 0.01 part of dodecenylsuccinic acid, viscosity
5 parts of index improver, 0.01 part of defoaming agent;
(2) functionalization cottonseed oil is added in reconciliation kettle, bis- (2- ethylhexyl) last of the ten Heavenly stems two is added at being 70 DEG C in temperature
Acid esters, dispersing agent, extreme pressure anti-wear additives, dodecenylsuccinic acid, potassium sorbate stir 15min, antioxidant then are added, viscosity refers to
Number modifier, defoaming agent stir 40min, are released by 5 μm of filters to get Biodegradable lubricant oil.
The revolving speed stirred in the step (2) is 500r/min.
The functionalization cottonseed oil the preparation method comprises the following steps: being in mass ratio that 1:0.09 is with revolving speed by cottonseed oil, ethyl alcohol
Being 40 DEG C in environment temperature after 300r/min stirring 10min uses radiation dose rate to be irradiated for the 60Co gamma-rays of 5kGy/h
3h is handled, then temperature is 50 DEG C, absolute pressure is 0.006MPa vacuum distillation removal ethyl alcohol, cottonseed after being irradiated
Oil;It is in mass ratio by the cottonseed oil after irradiation, acetic acid, isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters, concentrated phosphoric acid
1:0.09:0.09:0.004 with revolving speed be 300r/min stir 10min, temperature be 40 DEG C, revolving speed be 300r/min stirring under
40wt% hydrogen peroxide is added dropwise, the rate of addition of the 40wt% hydrogen peroxide is 0.2g/s, and the dosage of the 40wt% hydrogen peroxide is
30% of cottonseed oil weight after irradiation after hydrogen peroxide is added dropwise, is warming up to 60 DEG C of reaction 4h, and liquid separation removes water phase, obtains
Reaction product;Reaction product is carried out being washed to pH being 7 with the sodium hydrate aqueous solution of 0.6wt%, the reaction after washing is produced
Object is 75 DEG C, absolute pressure 0.006MPa vacuum dehydration 2.5h in temperature, obtains functionalization cottonseed oil.
The dispersing agent is boronation polyisobutylene succinamide.
The antioxidant is 2,6 di tert butyl 4 methyl phenol.
The viscosity index improver is polymethacrylates.
The extreme pressure anti-wear additives are different octyloxy (tridecyl primene JM-T benzotriazole) phosphate derivative.
The defoaming agent is polyether-modified silicon defoaming agent.
Comparative example 1
The preparation method of Biodegradable lubricant oil, includes the following steps:
(1) each raw material: 70 parts of functionalization cottonseed oil, bis- (2- ethylhexyl) sebacate 10 part, points is weighed by weight
0.5 part of powder, 3 parts of extreme pressure anti-wear additives, 1.5 parts of antioxidant, 0.01 part of potassium sorbate, 0.01 part of dodecenylsuccinic acid, viscosity
5 parts of index improver, 0.01 part of defoaming agent;
(2) functionalization cottonseed oil is added in reconciliation kettle, bis- (2- ethylhexyl) last of the ten Heavenly stems two is added at being 70 DEG C in temperature
Acid esters, dispersing agent, extreme pressure anti-wear additives, dodecenylsuccinic acid, potassium sorbate stir 15min, antioxidant then are added, viscosity refers to
Number modifier, defoaming agent stir 40min, are released by 5 μm of filters to get Biodegradable lubricant oil.
The revolving speed stirred in the step (2) is 500r/min.
The functionalization cottonseed oil the preparation method comprises the following steps: being in mass ratio that 1:0.09 is with revolving speed by cottonseed oil, ethyl alcohol
It is 40 DEG C of isothermal holding 3h that 300r/min, which is stirred after 10min in environment temperature, then temperature is 50 DEG C, absolute pressure is
0.006MPa vacuum distillation removal ethyl alcohol, the cottonseed oil after being irradiated;By cottonseed oil, acetic acid, the isopropyl three (two after irradiation
Octyl pyrophosphoric acid acyloxy) titanate esters, concentrated phosphoric acid be in mass ratio 1:0.09:0.09:0.004 with revolving speed be 300r/min stirring
10min, temperature be 40 DEG C, revolving speed be 300r/min stirring under be added dropwise 40wt% hydrogen peroxide, the drop of the 40wt% hydrogen peroxide
Acceleration is 0.2g/s, and the dosage of the 40wt% hydrogen peroxide is 30% of the cottonseed oil weight after irradiation, and hydrogen peroxide drips
Bi Hou, is warming up to 60 DEG C of reaction 4h, and liquid separation removes water phase, obtains reaction product;By the sodium hydroxide of reaction product 0.6wt%
It is 7 that aqueous solution, which be washed to pH, in temperature is 75 DEG C, absolute pressure 0.006MPa vacuum dehydration by the reaction product after washing
2.5h obtains functionalization cottonseed oil.
The dispersing agent is boronation polyisobutylene succinamide.
The antioxidant is 2,6 di tert butyl 4 methyl phenol.
The viscosity index improver is polymethacrylates.
The extreme pressure anti-wear additives are different octyloxy (tridecyl primene JM-T benzotriazole) phosphate derivative.
The defoaming agent is polyether-modified silicon defoaming agent.
Comparative example 2
The preparation method of Biodegradable lubricant oil, includes the following steps:
(1) each raw material: 70 parts of functionalization cottonseed oil, bis- (2- ethylhexyl) sebacate 10 part, points is weighed by weight
0.5 part of powder, 3 parts of extreme pressure anti-wear additives, 1.5 parts of antioxidant, 0.01 part of potassium sorbate, 0.01 part of dodecenylsuccinic acid, viscosity
5 parts of index improver, 0.01 part of defoaming agent;
(2) functionalization cottonseed oil is added in reconciliation kettle, bis- (2- ethylhexyl) last of the ten Heavenly stems two is added at being 70 DEG C in temperature
Acid esters, dispersing agent, extreme pressure anti-wear additives, dodecenylsuccinic acid, potassium sorbate stir 15min, antioxidant then are added, viscosity refers to
Number modifier, defoaming agent stir 40min, are released by 5 μm of filters to get Biodegradable lubricant oil.
The revolving speed stirred in the step (2) is 500r/min.
The functionalization cottonseed oil the preparation method comprises the following steps: being in mass ratio that 1:0.09 is with revolving speed by cottonseed oil, ethyl alcohol
Being 40 DEG C in environment temperature after 300r/min stirring 10min uses radiation dose rate to be irradiated for the 60Co gamma-rays of 5kGy/h
3h is handled, then temperature is 50 DEG C, absolute pressure is 0.006MPa vacuum distillation removal ethyl alcohol, cottonseed after being irradiated
Oil;It is in mass ratio 1:0.09:0.004 with revolving speed by the cottonseed oil after irradiation, acetic acid, concentrated phosphoric acid is 300r/min stirring
10min, temperature be 40 DEG C, revolving speed be 300r/min stirring under be added dropwise 40wt% hydrogen peroxide, the drop of the 40wt% hydrogen peroxide
Acceleration is 0.2g/s, and the dosage of the 40wt% hydrogen peroxide is 30% of the cottonseed oil weight after irradiation, and hydrogen peroxide drips
Bi Hou, is warming up to 60 DEG C of reaction 4h, and liquid separation removes water phase, obtains reaction product;By the sodium hydroxide of reaction product 0.6wt%
It is 7 that aqueous solution, which be washed to pH, in temperature is 75 DEG C, absolute pressure 0.006MPa vacuum dehydration by the reaction product after washing
2.5h obtains functionalization cottonseed oil.
The dispersing agent is boronation polyisobutylene succinamide.
The antioxidant is 2,6 di tert butyl 4 methyl phenol.
The viscosity index improver is polymethacrylates.
The extreme pressure anti-wear additives are different octyloxy (tridecyl primene JM-T benzotriazole) phosphate derivative.
The defoaming agent is polyether-modified silicon defoaming agent.
Comparative example 3
The preparation method of Biodegradable lubricant oil, includes the following steps:
(1) each raw material: 70 parts of functionalization cottonseed oil, bis- (2- ethylhexyl) sebacate 10 part, points is weighed by weight
0.5 part of powder, 3 parts of extreme pressure anti-wear additives, 1.5 parts of antioxidant, 0.01 part of potassium sorbate, 0.01 part of dodecenylsuccinic acid, viscosity
5 parts of index improver, 0.01 part of defoaming agent;
(2) functionalization cottonseed oil is added in reconciliation kettle, bis- (2- ethylhexyl) last of the ten Heavenly stems two is added at being 70 DEG C in temperature
Acid esters, dispersing agent, extreme pressure anti-wear additives, dodecenylsuccinic acid, potassium sorbate stir 15min, antioxidant then are added, viscosity refers to
Number modifier, defoaming agent stir 40min, are released by 5 μm of filters to get Biodegradable lubricant oil.
The revolving speed stirred in the step (2) is 500r/min.
The functionalization cottonseed oil the preparation method comprises the following steps: by cottonseed oil, acetic acid, (the dioctylphyrophosphoric acid acyl-oxygen of isopropyl three
Base) titanate esters, concentrated phosphoric acid be in mass ratio 1:0.09:0.09:0.004 with revolving speed be 300r/min stirring 10min, be in temperature
40 DEG C, revolving speed is that 300r/min stirring is lower that 40wt% hydrogen peroxide is added dropwise, the rate of addition of the 40wt% hydrogen peroxide is 0.2g/s,
The dosage of the 40wt% hydrogen peroxide is the 30% of cottonseed oil weight, after hydrogen peroxide is added dropwise, is warming up to 60 DEG C of reaction 4h, point
Liquid removes water phase, obtains reaction product;Reaction product is carried out being washed to pH being 7 with the sodium hydrate aqueous solution of 0.6wt%, it will
Reaction product after washing is 75 DEG C, absolute pressure 0.006MPa vacuum dehydration 2.5h in temperature, obtains functionalization cottonseed oil.
The dispersing agent is boronation polyisobutylene succinamide.
The antioxidant is 2,6 di tert butyl 4 methyl phenol.
The viscosity index improver is polymethacrylates.
The extreme pressure anti-wear additives are different octyloxy (tridecyl primene JM-T benzotriazole) phosphate derivative.
The defoaming agent is polyether-modified silicon defoaming agent.
Embodiment 3
The preparation method of Biodegradable lubricant oil, includes the following steps:
(1) each raw material: 70 parts of functionalization cottonseed oil, bis- (2- ethylhexyl) sebacate 10 part, points is weighed by weight
0.5 part of powder, 3 parts of extreme pressure anti-wear additives, 1.5 parts of antioxidant, 0.01 part of potassium sorbate, 0.01 part of dodecenylsuccinic acid, viscosity
5 parts of index improver, 0.01 part of defoaming agent;
(2) functionalization cottonseed oil is added in reconciliation kettle, bis- (2- ethylhexyl) last of the ten Heavenly stems two is added at being 70 DEG C in temperature
Acid esters, dispersing agent, extreme pressure anti-wear additives, dodecenylsuccinic acid, potassium sorbate stir 15min, antioxidant then are added, viscosity refers to
Number modifier, defoaming agent stir 40min, are released by 5 μm of filters to get Biodegradable lubricant oil.
The revolving speed stirred in the step (2) is 500r/min.
The functionalization cottonseed oil the preparation method comprises the following steps: being in mass ratio that 1:0.09 is with revolving speed by cottonseed oil, ethyl alcohol
Being 40 DEG C in environment temperature after 300r/min stirring 10min uses radiation dose rate to be irradiated for the 60Co gamma-rays of 5kGy/h
3h is handled, then temperature is 50 DEG C, absolute pressure is 0.006MPa vacuum distillation removal ethyl alcohol, cottonseed after being irradiated
Oil;It is in mass ratio by the cottonseed oil after irradiation, acetic acid, isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters, concentrated phosphoric acid
1:0.09:0.09:0.004 with revolving speed be 300r/min stir 10min, temperature be 40 DEG C, revolving speed be 300r/min stirring under
40wt% hydrogen peroxide is added dropwise, the rate of addition of the 40wt% hydrogen peroxide is 0.2g/s, and the dosage of the 40wt% hydrogen peroxide is
30% of cottonseed oil weight after irradiation after hydrogen peroxide is added dropwise, is warming up to 60 DEG C of reaction 4h, and liquid separation removes water phase, obtains
Reaction product;Reaction product is carried out being washed to pH being 7 with the sodium hydrate aqueous solution of 0.6wt%, the reaction after washing is produced
Object is 75 DEG C, absolute pressure 0.006MPa vacuum dehydration 2.5h in temperature, obtains functionalization cottonseed oil.
The dispersing agent is boronation polyisobutylene succinamide.
The antioxidant is 2,6 di tert butyl 4 methyl phenol.
The viscosity index improver is polymethacrylates.
The extreme pressure anti-wear additives are n-butoxy (cyclohexylamine methyl benzotriazole) phosphate derivative.
The defoaming agent is polyether-modified silicon defoaming agent.
Embodiment 4
The preparation method of Biodegradable lubricant oil, includes the following steps:
(1) each raw material: 70 parts of functionalization cottonseed oil, bis- (2- ethylhexyl) sebacate 10 part, points is weighed by weight
0.5 part of powder, 3 parts of extreme pressure anti-wear additives, 1.5 parts of antioxidant, 0.01 part of potassium sorbate, 0.01 part of dodecenylsuccinic acid, viscosity
5 parts of index improver, 0.01 part of defoaming agent;
(2) functionalization cottonseed oil is added in reconciliation kettle, bis- (2- ethylhexyl) last of the ten Heavenly stems two is added at being 70 DEG C in temperature
Acid esters, dispersing agent, extreme pressure anti-wear additives, dodecenylsuccinic acid, potassium sorbate stir 15min, antioxidant then are added, viscosity refers to
Number modifier, defoaming agent stir 40min, are released by 5 μm of filters to get Biodegradable lubricant oil.
The revolving speed stirred in the step (2) is 500r/min.
The functionalization cottonseed oil the preparation method comprises the following steps: being in mass ratio that 1:0.09 is with revolving speed by cottonseed oil, ethyl alcohol
Being 40 DEG C in environment temperature after 300r/min stirring 10min uses radiation dose rate to be irradiated for the 60Co gamma-rays of 5kGy/h
3h is handled, then temperature is 50 DEG C, absolute pressure is 0.006MPa vacuum distillation removal ethyl alcohol, cottonseed after being irradiated
Oil;It is in mass ratio by the cottonseed oil after irradiation, acetic acid, isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters, concentrated phosphoric acid
1:0.09:0.09:0.004 with revolving speed be 300r/min stir 10min, temperature be 40 DEG C, revolving speed be 300r/min stirring under
40wt% hydrogen peroxide is added dropwise, the rate of addition of the 40wt% hydrogen peroxide is 0.2g/s, and the dosage of the 40wt% hydrogen peroxide is
30% of cottonseed oil weight after irradiation after hydrogen peroxide is added dropwise, is warming up to 60 DEG C of reaction 4h, and liquid separation removes water phase, obtains
Reaction product;Reaction product is carried out being washed to pH being 7 with the sodium hydrate aqueous solution of 0.6wt%, the reaction after washing is produced
Object is 75 DEG C, absolute pressure 0.006MPa vacuum dehydration 2.5h in temperature, obtains functionalization cottonseed oil.
The dispersing agent is boronation polyisobutylene succinamide.
The antioxidant is 2,6 di tert butyl 4 methyl phenol.
The viscosity index improver is polymethacrylates.
The extreme pressure anti-wear additives are n-butoxy (cyclohexylamine methyl benzotriazole) phosphate derivative, different octyloxy (13
Alkyl primene JM-T benzotriazole) phosphate derivative is that 1:3 is mixed in mass ratio to obtain the final product.
The defoaming agent is polyether-modified silicon defoaming agent.
Test case 1
Wear-resistant test is carried out to the Biodegradable lubricant oil of embodiment preparation.Concrete outcome is shown in Table 1.
The wear-resistant test of high temperature: carrying out the wear-resistant test of high temperature of Biodegradable lubricant oil using SRV frictional testing machine,
Experimental condition is load 300N, frequency 50Hz, stroke 1mm, 120 DEG C of temperature.
Table 1: wear-resistant experimental test result table
Test case 2
Carrying out anti-oxidative stability to the Biodegradable lubricant oil that embodiment is prepared can test.Concrete outcome is shown in Table
2。
Anti-oxidative stability can be tested: according to measurement-rotary oxygen bomb of SH/T 0193-2008 lubricating oil oxidation stability
Method detection.
Table 2: anti-oxidative stability energy test data table
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (10)
1. a kind of preparation method of Biodegradable lubricant oil, which is characterized in that include the following steps:
(1) each raw material: cottonseed oil, bis- (2- ethylhexyl) sebacates, dispersing agent, extreme pressure anti-wear additives, antioxidant, sorb is weighed
Sour potassium, dodecenylsuccinic acid, viscosity index improver, defoaming agent;
(2) cottonseed oil is added to and is reconciled in kettle, stirring, by 2-10 μm of filter release to get.
2. the preparation method of Biodegradable lubricant oil as described in claim 1, which is characterized in that include the following steps:
(1) each raw material: cottonseed oil or 65-75 parts of functionalization cottonseed oil, bis- (2- ethylhexyl) sebacates is weighed by weight
5-15 parts, 0.2-1 parts of dispersing agent, 1-5 parts of extreme pressure anti-wear additives, 0.5-2.5 parts of antioxidant, 0.005-0.025 parts of potassium sorbate, ten
0.005-0.025 parts of dialkylene succinic acid, 3-9 parts of viscosity index improver, 0.005-0.025 parts of defoaming agent;
(2) cottonseed oil or functionalization cottonseed oil are added in reconciliation kettle, bis- (2- ethyl hexyls is added at being 65-75 DEG C in temperature
Base) sebacate, dispersing agent, extreme pressure anti-wear additives, dodecenylsuccinic acid, potassium sorbate stirring 10-20min, it is then added anti-
Oxygen agent, viscosity index improver, defoaming agent stir 30-50min, by 2-10 μm of filter release to get.
3. the preparation method of Biodegradable lubricant oil as claimed in claim 2, it is characterised in that: stirring in the step (2)
Revolving speed be 300-700r/min.
4. the preparation method of Biodegradable lubricant oil as claimed in claim 2, it is characterised in that: the functionalization cottonseed oil
The preparation method comprises the following steps: being in mass ratio 1:(0.07-0.12 by cottonseed oil, ethyl alcohol) with revolving speed be 100-500r/min stir 5-
Being 30-50 DEG C in environment temperature after 15min uses radiation dose rate to carry out radiation treatment 2- for the 60Co gamma-rays of 3-7kGy/h
5h, then temperature is 40-55 DEG C, absolute pressure is 0.005-0.01MPa vacuum distillation removal ethyl alcohol, cotton after being irradiated
Seed oil;By after irradiation cottonseed oil, acetic acid, isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters, concentrated phosphoric acid in mass ratio
For 1:(0.07-0.12), (0.07-0.12), (0.003-0.005) with revolving speed be 100-500r/min stir 5-15min, in temperature
Degree, which is 30-50 DEG C, revolving speed is that 100-500r/min stirring is lower is added dropwise 35-45wt% hydrogen peroxide, the 35-45wt% hydrogen peroxide
Rate of addition is 0.1-0.5g/s, and the dosage of the 35-45wt% hydrogen peroxide is the 30-35% of the cottonseed oil weight after irradiation,
After hydrogen peroxide is added dropwise, it is warming up to 55-65 DEG C of reaction 3-5h, liquid separation removes water phase, obtains reaction product;Reaction product is used
It is 6.5-7.5 that the sodium hydrate aqueous solution of 0.5-1wt%, which be washed to pH, in temperature is 70- by the reaction product after washing
80 DEG C, absolute pressure 0.005-0.01MPa vacuum dehydration 2-5h, obtain functionalization cottonseed oil.
5. the preparation method of Biodegradable lubricant oil as claimed in claim 2, it is characterised in that: the dispersing agent is poly- isobutyl
Alkenyl succimide and/or boronation polyisobutylene succinamide.
6. the preparation method of Biodegradable lubricant oil as claimed in claim 2, it is characterised in that: the antioxidant is 2,6- bis-
Tert-butyl-4-methyl-Phenol or 4- amino -2,6 di t butyl phenol.
7. the preparation method of Biodegradable lubricant oil as claimed in claim 2, it is characterised in that: the viscosity index improver
For polymethacrylates.
8. the preparation method of Biodegradable lubricant oil as claimed in claim 2, it is characterised in that: the extreme pressure anti-wear additives are positive
Butoxy (cyclohexylamine methyl benzotriazole) phosphate derivative and/or different octyloxy (tridecyl primene JM-T benzotriazole) phosphoric acid
Ester derivant.
9. the preparation method of Biodegradable lubricant oil as claimed in claim 2, it is characterised in that: the defoaming agent changes for polyethers
Property silicon defoaming agent.
10. a kind of Biodegradable lubricant oil, using the preparation of Biodegradable lubricant oil described in any one of claim 1-9
Method is prepared.
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